CN106087037A - Crystal pull growth furnace temperature field structure and pulling growth technique thereof - Google Patents
Crystal pull growth furnace temperature field structure and pulling growth technique thereof Download PDFInfo
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- CN106087037A CN106087037A CN201610760201.0A CN201610760201A CN106087037A CN 106087037 A CN106087037 A CN 106087037A CN 201610760201 A CN201610760201 A CN 201610760201A CN 106087037 A CN106087037 A CN 106087037A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/14—Heating of the melt or the crystallised materials
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Abstract
The invention discloses a kind of crystal pull growth furnace temperature field structure and pulling growth technique thereof, temperature field structure includes being incubated insulation urceolus (9) on inner core (8) and zirconium oxide on aluminium oxide heat-preservation cylinder (1), zirconia brick heat-preservation cylinder (2), iridium crucible (3), zirconium oxide crucible torr (4), aluminium oxide collet (5), the first zirconium oxide cover plate (6), the second zirconium oxide cover plate (13), aluminium oxide locating ring (7), aluminium oxide；Technique includes: prepare before shove charge, processes iridium crucible, shove charge, charging, for the first time material, seed crystal preparation and adjusting, for the second time material, inflate, preheat seed crystal, crystal growth, ending.The present invention devises reasonably temperature field structure and growth technique, reduces energy consumption on the premise of ensureing the required high temperature of growth and thermograde.Carry out necking down before shouldering, i.e. start to make temperature the most higher when lifting, allow seed crystal diameter micro-receipts about about 1mm, shouldering of lowering the temperature the most again, it is possible to reduce seed crystal defect as far as possible and extend to inside crystal.
Description
Technical field
The present invention relates to field of crystal growth, particularly relate to a kind of crystal pull growth furnace temperature field structure and lifting is raw
Long technique.
Background technology
Czochralski method also known as Czoncharlski method, be Czochralski (J.Czochralski) invention in 1917 from molten
The method of pulling growth high quality single crystal in body.This method can grow colourless sapphire, ruby, yttrium pyralspite, gadolinium gallium
The important gem crystals such as garnet, alexandrite and spinelle.
The ultimate principle of czochralski method: czochralski method is to be placed on the raw material constituting crystal in crucible to add heat fusing, at melt table
Face connects seed crystal lifting melt, under controlled conditions, makes seed crystal and melt constantly carry out atom or molecule on interface again
Arrangement, gradually solidifies with cooling and grows monocrystal.First the raw material of crystal to be grown is put by the growth technique of czochralski method
In resistant to elevated temperatures crucible, add heat fusing, adjust temperature field in furnace, make melt top be in supercooled state；Then at seedholder
On lay a seed crystal, allow seed crystal contact bath surface, after seed crystal face is slightly molten, lifts and rotate iridium bar, make melt be in
Supercooled state and crystallize on seed crystal, in constantly lifting and rotary course, grow cylinder crystal.
The process of a kind of crystallization that the growth of laser crystal is mainly carried out under conditions of high-temperature fusion, owing to growth is wanted
Ask temperature higher, and the method obtaining high temperature is Frequency Induction Heating, therefore the consumption to electric energy is higher.Yet with itself
The process of crystallization needs certain thermograde difference, so needing certain thermal loss to form a certain amount of temperature ladder
Degree difference, thus ensure the stability of crystallization process.Warm field structure the most reasonable in design and pulling growth technique, ensureing
Reduce energy consumption and cost on the premise of high temperature needed for pulling growth and thermograde, become problem demanding prompt solution.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of crystal pull growth furnace temperature field structure and
Pulling growth technique, reduces energy consumption and cost on the premise of the high temperature ensured needed for pulling growth and thermograde.
It is an object of the invention to be achieved through the following technical solutions: crystal pull growth furnace temperature field structure, including oxygen
Change aluminum heat-preservation cylinder, zirconia brick heat-preservation cylinder, iridium crucible, zirconium oxide crucible torr, aluminium oxide collet, the first zirconium oxide cover plate, aluminium oxide are fixed
It is incubated on inner core and zirconium oxide on position ring, aluminium oxide and is incubated urceolus；The perisporium of iridium crucible is incubated by zirconia brick the most successively
Cylinder and aluminium oxide heat-preservation cylinder are coated with；It is located at the bottom of the crucible of iridium crucible in zirconium oxide crucible torr, zirconium oxide crucible torr, zirconia brick heat-preservation cylinder and oxygen
Change aluminum heat-preservation cylinder support respectively on aluminium oxide collet；The top open part of iridium crucible is provided with the first zirconium oxide cover plate, the first oxidation
It is provided with aluminium oxide locating ring between zirconium cover plate and aluminium oxide heat-preservation cylinder, aluminium oxide is incubated insulation urceolus on inner core and zirconium oxide and divides
It is not arranged on the first zirconium oxide cover plate, and on zirconium oxide, insulation urceolus is located at aluminium oxide locating ring and insulation inner core on aluminium oxide
Between；The second zirconium oxide cover plate that is also arranged above being incubated urceolus on inner core and zirconium oxide it is incubated on described aluminium oxide, described
Aluminium oxide on be incubated on inner core and zirconium oxide and be incubated urceolus and be the heat-preservation cylinder of reduction thickness.
The ratio of insulation urceolus reduction thickness on inner core and zirconium oxide that is incubated on described aluminium oxide is 30%-50%.
Crystal pull growth furnace temperature field structure, also includes induction coil, and the upper edge of iridium crucible exceeds 1 than edge on induction coil dead ahead
~ 3mm, aluminium oxide heat-preservation cylinder is higher than induction coil 30 ~ 32mm.
The upper edge of described iridium crucible than on zirconia brick heat-preservation cylinder along low 5 ~ 8mm.
Described aluminium oxide locating ring is provided with foamed brick, and foamed brick is coated on zirconium oxide the outside being incubated urceolus.
Crystal pull growth furnace temperature field structure, also includes observation panel, and observation panel is located at the top of temperature field structure.
Crystal pull growth technique, comprises the following steps:
S1: prepare before shove charge；
S2: process iridium crucible；
S3: shove charge, charging, including following sub-step:
S301: the induction furnace to new clothes, first adjusts the levelness of induction coil, and the concentricity of induction coil and seed rod, partially
Difference should be less than 2mm；
S302: according to temperature field structure assembling temperature field, when dress temperature field, all of insulation material need to clean up without airborne dust, nothing
Temperature field can be loaded after falling slag；Adjust the concentricity of aluminium oxide heat-preservation cylinder, iridium crucible and seed rod, deviation≤1mm；
S303: after clearing furnace, fire door is shut, prepares charging；
Before charging, the foreign material in cleaning iridium crucible, prevent foreign material from directly contacting with material, iridium crucible；
Charging process wears altex glove, prevents secondary pollution；
After material installs, with swept be incubated on the first zirconium oxide cover plate of clean dust, the second zirconium oxide cover plate and aluminium oxide inner core,
It is incubated urceolus on zirconium oxide and installs heat-insulation system, adjust observation panel angle, and with on treated YAG crystal wafer lid；
Check again for induction coil with or without leaking, turn-to-turn short circuit, clean banking door after burner hearth, evacuation；
S4: material for the first time, including following sub-step:
S401: start mechanical pump, slowly open vacuum valve, after vacuum is evacuated to 5Pa, opens intermediate frequency power supply, manually rises Continental Europe table
OP to 80V, rises DC voltage to 100V to DC voltage after 1h；
S402: be heated to 100V, after vacuum is evacuated to 5Pa again, closes vacuum valve, closes mechanical pump, manually by Continental Europe OP
After value is down to 0, starts to be filled with argon extremely-0.01MPa, more manually rise the show value before the extremely inflation of Continental Europe OP value；
S403: entering automatic heating program, heating rate is 1.2mv/h, until material is smashed, now EF power is 11-
15KW；
S404: after material is smashed, is cooled to after 0.5mv close intermediate frequency with the speed of-1.2mv/h, and after 12 hours, blow-on door prepares the
Secondary material；
The preparation of S5: seed crystal and adjustment, including following sub-step:
S501: seed crystal garnet crystal orients through strict, and deviation is less than 1 °, the side's of being cut into bar；
S502: grind a symmetrical parallel semicircle sulculus with boron carbide fine sand two sides at one end 6-8mm of seed crystal, make seed crystal
It is contained on iridium bar vertical and has a little loosening；
S503: after seed crystal milled, uses gasoline wash clean, then cleans with acetone, then adds detergent with tap water and cleans；Use after complete
The dilute hydrochloric acid of 1:5 soaks 5-10min, takes out and uses recycled water wash clean, and with available after alcohol wipe；
After S504: the second defective material installs, load onto seed crystal and mix up the concentricity of seed crystal, Concentricity tolerance≤1mm, weight fluctuation ＜
0.2-0.5g；
After S505: seed crystal adjusts, adjust the viewing angle of observation panel, clean up burner hearth, banking door, evacuation, prepare the
Secondary material；
S6: for the second time material, inflate, preheat seed crystal, including following sub-step:
S601: the evacuation of material, inflation, temperature increasing for melting materials process have all operated with reference to material for the first time for the second time, heat up speed
Rate is 0.6mv/h；
S602: when Continental Europe table shows to 9mv, stops heating, opens mechanical pump evacuation, when being evacuated to-0.1MPa, stops taking out very
Sky, is filled with argon to 0.01MPa, then proceedes to heat up with 0.6mv/h, until material is completely melt；
S603: material needs to preheat seed crystal simultaneously, and the manual sinking seed crystal 2.5mm every 5 minutes, until seed crystal chaotropic face 1-2mm；
S7: crystal growth, including following sub-step:
S701: sow, including:
S7011: constant temperature 0.5-1h after materialization is complete, then manually under shake seed crystal and sow, allow seed crystal contact with liquid level；
Start homoiothermic after S7012: seed crystal contact liquid level, carry out homoiothermic, constant temperature after each homoiothermic according to melt situation actual in stove
20min, and observe seed crystal head situation of change, when seed crystal head shrinks slightly, and contact formation half inverted cone-shaped with liquid level, and protect always
When holding constant, show that temperature adjusts suitable；
S7013: temperature adjust suitable after, point 3 sinking seed crystal 2mm, each interval time 10-20min, sink seed for the last time
Constant temperature 0.5-1h after brilliant 0.5mm, can open and draw, rotating speed: 8-12 rev/min, pulling rate: 0.5-1mm/h；
S702: necking down: when starting to lift, makes temperature the most higher, allows seed crystal diameter micro-receipts about 1mm, entrance of lowering the temperature the most again
Shouldering；
S703: shouldering, isometrical, including:
The complete rear constant temperature 1h of S7031: necking down, setting speed: 8-12 rev/min, pulling rate: 0.5-1mm/h；
S7032: in observation stove, crystal situation and crystal diameter and setting value walk power curve, if two curve deviations are little or crystal
Diametral curve is in slow shouldering state, can enter Automatic Control after inputting process parameters；
S7033: entering after automatically controlling, shouldering, isodiametric growth are grown by procedure auto-control temperature, and shouldering angle is
15-26 °, crystal diameter is 23-26 ° before φ 28mm, for 15-18 ° after reaching φ 28mm, proceed to isometrical after be 0 °；
S7034: when isodiametric growth to predetermined length, enters finishing phase；
S8: ending.
Described step S1 includes that brilliant liter/brilliant turning checks that step, weighing system check that step, vacuum check step, water route
With channel check step, Continental Europe systems inspection step, induction coil check step and mechanical pump check in step any one or
Multiple combination:
(1) brilliant liter/crystalline substance turn checks: the brilliant liter of detection, crystalline substance turn the most properly functioning, and fluctuation of speed scope is normal ± 0.1, pulling rate
Fluctuation range is normal ± 0.01, and crystalline substance turns non-jitter, and brilliant liter is without creeping phenomenon；
(2) weighing system inspection: detection weighing system is the most properly functioning, and weight fluctuation ＜ 0.2g is normal；
(3) vacuum inspection, including following sub-step:
SS1: closed furnace door, checks whether venting valve, charging valve close；
SS2: start mechanical pump, slowly open vacuum valve；
SS3: observe vacuometer, whether detection furnace pressure can reach below 5Pa, and maintain a period of time；
(4) water route and channel check: check whether each cooling water channel is opened before starting the heating, hydraulic pressure is the most normal: body of heater water
Pressure is 0.04-0.06MPa, and induction coil hydraulic pressure is 0.25-0.3MPa；Check circuit whether normal operation；
(5) Continental Europe systems inspection: logical upper Continental Europe power supply, Continental Europe table, to automatically, arranges auto linear heating schedule, and observation program is
No properly functioning, Continental Europe table mv value displays whether normally；
(6) induction coil inspection: check whether induction coil leaks, with or without the phenomenon of turn-to-turn short circuit；
(7) mechanical pump inspection: check whether the oil of mechanical pump adds properly, in terms of observation panel, oil is added to the half of observation panel；
Open mechanical pump power supply, see that operating is the most normal.
Described step S2 includes following sub-step:
S201: after the dilute hydrochloric acid of use 1:5 is to cleaning 0.5-1h inside and outside iridium crucible, cleans up with distilled water and dry, and use ethanol
Wiped clean is standby；
Carrying out vacuum sky burning before the charging of S202: iridium crucible to process, vacuum sky burning processes and includes following sub-step:
S2021: mix up the concentricity rear enclosed fire door of iridium crucible and seed rod, closes venting valve；
S2022: start mechanical pump, slowly opens vacuum valve, starts evacuation；
S2023: after vacuum is evacuated to 5Pa, starts intermediate frequency power supply, first opens control loop, opens major loop again, manually rises Continental Europe table OP value
To DC voltage to 80V；After 1h, liter DC voltage is to 100V, utilizes JPG Automatic Program to heat up, heating rate after half an hour
For 1.2mv/h；
S2024: observe iridium crucible sky in stove and burn situation, when with the naked eye watching iridium crucible and feeling the most dazzling, stopping heating up enters constant temperature
State, now EF power about 7-8KW；After constant temperature 2h, starting cooling automatically, rate of temperature fall is-1.2mv/h, is cooled to 0.5mv
Intermediate frequency power supply can be closed, close mechanical pump；
S2025: closing intermediate frequency power supply order: Continental Europe furnishing is manual, OP value is down to 0, closes major loop, closes and controls loop, closes power supply
Plug-in strip；
S2026: fire door can be opened after closing intermediate frequency power supply 12h.
The step being filled with argon described in step S402 includes:
S4021: charging valve is unscrewed, then open gas cylinder valve；
S4022: slowly charging valve is progressively tightened, first aerofluxus, after being emptied by the air in connecting tube, reconnect inflation air inlet
Pipe；
S4023: slowly open inflation connecting valve, after making stove internal gas pressure rise to specify air pressure, first closes inflation connecting valve,
Turn off gas cylinder valve, the most again charging valve is unscrewed；
S4024: pull down connecting tube, shifts home onto gas cylinder dolly.
The invention has the beneficial effects as follows:
1) it is incubated the top of urceolus on insulation inner core and zirconium oxide on alumina and sets up zirconium oxide cover plate, can effectively strengthen temperature
The heat insulation effect of field, it is possible to reduce the power consumption of 5%-10%；But the problem that the enhancing of Wen Chang upper strata heat insulation effect brings is cannot
Form the thermograde needed for crystal growth, it is contemplated that this problem, by outside insulation on insulation inner core on aluminium oxide and zirconium oxide
Reduced down in thickness 30%-50% of cylinder, to improve the temperature difference, reaches the thermograde needed for crystal growth, reduces heat-preservation cylinder material simultaneously
Material cost.Devise reasonably temperature field structure and pulling growth technique, in the high temperature ensured needed for pulling growth and thermograde
On the premise of reduce energy consumption and cost.
2) iridium crucible first passes through dilute hydrochloric acid scouring before charging, cleaner by wipes of alcohol after distilled water cleans and dries, permissible
Effectively remove the metal in iridium crucible, metal oxide impurities；Iridium crucible carries out vacuum sky burning in addition process, can effectively remove iridium
The combustibles such as the oils and fats in crucible, organic impurities, it is ensured that the cleanliness factor of iridium crucible.
3) add detergent clean with gasoline, acetone, tap water before and after after seed crystal milled, then use regeneration after dilute hydrochloric acid immersion
Water cleans, and by alcohol wipe, it is ensured that the cleannes of seed crystal, thus ensure that crystal quality.
4) the strict speed controlling material fusing during material, prevents from heating up too fast too high；Meanwhile, under strict control once
The distance of heavy seed crystal, can effectively prevent seed crystal preheating uneven and burst.
5), after seed crystal contact liquid level, according to melt situation homoiothermic actual in stove, when seed crystal head shrinks slightly, and connect with liquid level
Touch and form half inverted cone-shaped, and when being always maintained at constant, show that temperature adjusts suitable, guarantee to sow by the way of this dynamic temperature-regulating
During temperature controlled accuracy.
6) before shouldering, there is a necking process, when i.e. starting to lift, make temperature the most higher, allow the micro-receipts of seed crystal diameter
About about 1mm, cooling enters shouldering the most again, it is possible to reduces seed crystal defect as far as possible and extends to inside crystal.
Accompanying drawing explanation
Fig. 1 is temperature field structure schematic diagram of the present invention；
Fig. 2 is that the present invention sows different temperatures seeding down crystal-tipped state vs's schematic diagram in step；
In figure, 1-aluminium oxide heat-preservation cylinder, 2-zirconia brick heat-preservation cylinder, 3-iridium crucible, 4-zirconium oxide crucible torr, 5-aluminium oxide collet, 6-
First zirconium oxide cover plate, 7-aluminium oxide locating ring, 8-aluminium oxide is incubated inner core, 9-zirconium oxide is incubated urceolus, 10-foam
Brick, 11-observation panel, 12-induction coil, 13-the second zirconium oxide cover plate.
Detailed description of the invention
Technical scheme is described in further detail below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to
The following stated.
As it is shown in figure 1, crystal pull growth furnace temperature field structure, including aluminium oxide heat-preservation cylinder 1, zirconia brick heat-preservation cylinder 2, iridium
Inner core 8 and it is incubated on crucible 3, zirconium oxide crucible torr 4, aluminium oxide collet the 5, first zirconium oxide cover plate 6, aluminium oxide locating ring 7, aluminium oxide
Urceolus 9 it is incubated on zirconium oxide；The perisporium of iridium crucible 3 is wrapped by zirconia brick heat-preservation cylinder 2 and aluminium oxide heat-preservation cylinder 1 the most successively
Cover；It is located at the bottom of the crucible of iridium crucible 3 in zirconium oxide crucible torr 4, zirconium oxide crucible torr 4, zirconia brick heat-preservation cylinder 2 and aluminium oxide heat-preservation cylinder 1 point
Other support is on aluminium oxide collet 5；The top open part of iridium crucible 3 is provided with the first zirconium oxide cover plate 6, the first zirconium oxide cover plate 6 with
It is provided with aluminium oxide locating ring 7 between aluminium oxide heat-preservation cylinder 1, aluminium oxide is incubated insulation urceolus 9 on inner core 8 and zirconium oxide and sets respectively
It is placed on the first zirconium oxide cover plate 6, and on zirconium oxide, insulation urceolus 9 is located at aluminium oxide locating ring 7 and insulation inner core 8 on aluminium oxide
Between；Be incubated on described aluminium oxide on inner core 8 and zirconium oxide be incubated urceolus 9 be also arranged above the second zirconium oxide cover plate 13,
It is incubated insulation urceolus 9 on inner core 8 and zirconium oxide on described aluminium oxide and is the heat-preservation cylinder of reduction thickness, the ratio of reduction thickness
For 30%-50%.
Crystal pull growth furnace temperature field structure, also includes induction coil 12, and the upper edge of iridium crucible 3 is than edge on induction coil 12 dead ahead
Exceed 1 ~ 3mm, aluminium oxide heat-preservation cylinder 1 30 ~ 32mm higher than induction coil 12.
The upper edge of described iridium crucible 3 than on zirconia brick heat-preservation cylinder 2 along low 5 ~ 8mm.
Described aluminium oxide locating ring 7 is provided with foamed brick 10, and foamed brick 10 is coated on zirconium oxide outside insulation urceolus 9
Side.
Crystal pull growth furnace temperature field structure, also includes that observation panel 11, observation panel 11 are located at the top of temperature field structure.
Crystal pull growth technique, comprises the following steps:
S1: prepare before shove charge, including brilliant rising/brilliant turn check step, weighing system check step, vacuum check step, water route and
Channel check step, Continental Europe systems inspection step, induction coil inspection step and mechanical pump inspection step:
(1) brilliant liter/crystalline substance turn inspection: the brilliant liter of detection, crystalline substance turn run the most normally.Actual measured value should be protected substantially with instrument indicated value
Hold consistent, and stable movement, fluctuation of speed scope is normal ± 0.1, and pulling rate fluctuation range is normal ± 0.01；And brilliant turn
Non-jitter, brilliant liter is without creeping phenomenon.
(2) weighing system inspection: detection weighing system is the most properly functioning, and weight fluctuation ＜ 0.2g is normal.
(3) vacuum inspection, including following sub-step:
SS1: closed furnace door, checks whether venting valve, charging valve close；
SS2: start mechanical pump, slowly open vacuum valve；
SS3: observe vacuometer, whether detection furnace pressure can reach below 5Pa, and maintain a period of time.
(4) water route and channel check: check whether each cooling water channel is opened before starting the heating, hydraulic pressure is the most normal: stove
Body hydraulic pressure is 0.04-0.06MPa, and induction coil hydraulic pressure is 0.25-0.3MPa；Check circuit whether normal operation.
(5) Continental Europe systems inspection: logical upper Continental Europe power supply, Continental Europe table to automatically, arranges auto linear heating schedule, observes journey
Sequence is the most properly functioning, and Continental Europe table mv value displays whether normally.
(6) induction coil inspection: check whether induction coil leaks, with or without the phenomenon of turn-to-turn short circuit.
(7) mechanical pump inspection: check whether the oil of mechanical pump adds properly, in terms of observation panel, oil is added to the half of observation panel
?；Open mechanical pump power supply, see that operating is the most normal.
S2: process iridium crucible, including following sub-step:
S201: after the dilute hydrochloric acid of use 1:5 is to cleaning 0.5-1h inside and outside iridium crucible, cleans up with distilled water and dry, and use ethanol
Wiped clean is standby；
Carrying out vacuum sky burning before the charging of S202: iridium crucible to process, vacuum sky burning processes and includes following sub-step:
S2021: mix up the concentricity rear enclosed fire door of iridium crucible and seed rod, closes venting valve；
S2022: start mechanical pump, slowly opens vacuum valve, starts evacuation；
S2023: after vacuum is evacuated to 5Pa, starts intermediate frequency power supply, first opens control loop, opens major loop again, manually rises Continental Europe table OP value
To DC voltage to 80V；After 1h, liter DC voltage is to 100V, utilizes JPG Automatic Program to heat up, heating rate after half an hour
For 1.2mv/h；
S2024: observe iridium crucible sky in stove and burn situation, when with the naked eye watching iridium crucible and feeling the most dazzling, stopping heating up enters constant temperature
State, now EF power about 7-8KW；After constant temperature 2h, starting cooling automatically, rate of temperature fall is-1.2mv/h, is cooled to 0.5mv
Intermediate frequency power supply can be closed, close mechanical pump；
S2025: closing intermediate frequency power supply order: Continental Europe furnishing is manual, OP value is down to 0, closes major loop, closes and controls loop, closes power supply
Plug-in strip；
S2026: fire door can be opened after closing intermediate frequency power supply 12h.
S3: shove charge, charging, including following sub-step:
S301: the induction furnace to new clothes, first adjusts the levelness of induction coil 12, and induction coil 12 and seed rod is concentric
Degree, deviation should be less than 2mm；
S302: assemble temperature field according to warm field structure as shown in Figure 1, when dress temperature field, all of insulation material need to use hairbrush, suction
Dirt device cleans up without airborne dust, without loading temperature field after falling slag；After installing temperature field, it should be ensured that crucible position error is at ± 3mm；Adjust
Whole good aluminium oxide heat-preservation cylinder 1, iridium crucible 3 and the concentricity of seed rod, deviation≤1mm；
S303: after clearing furnace, fire door is shut, prepares charging；
Before charging, glue the sand in clean iridium crucible 3 or other foreign material by clean alcohol gauze, prevent other metals and material, iridium
Crucible 3 directly contacts；
Charging process must wear altex glove, prevents secondary pollution, and whole process should complete as early as possible, simultaneously it should be noted that environment is grey
Dirt；
After material installs, with having swept on first zirconium oxide cover plate the 6, second zirconium oxide cover plate 13 of clean dust and aluminium oxide in insulation
Cylinder 8, zirconium oxide is incubated urceolus 9 installs heat-insulation system, adjust observation panel 11 angle, and with treated YAG crystal
Sheet covers；
Check again for induction coil 12 with or without leaking, turn-to-turn short circuit, with banking door after the clean burner hearth of vacuum, evacuation.
S4: material for the first time, including following sub-step:
S401: start mechanical pump, slowly open vacuum valve, after vacuum is evacuated to 5Pa, opens intermediate frequency power supply, manually rises Continental Europe table
OP to 80V, rises DC voltage to 100V to DC voltage after 1h；
S402: be heated to 100V, after vacuum is evacuated to 5Pa again, closes vacuum valve, closes mechanical pump, manually by Continental Europe OP
After value is down to 0, starts to be filled with argon extremely-0.01MPa, more manually rise the show value before the extremely inflation of Continental Europe OP value；
The step being filled with argon includes:
S4021: charging valve is unscrewed, then open gas cylinder valve；
S4022: slowly charging valve is progressively tightened, first aerofluxus, after being emptied by the air in connecting tube, reconnect inflation air inlet
Pipe；
S4023: slowly open inflation connecting valve, after making stove internal gas pressure rise to specify air pressure, first closes inflation connecting valve,
Turn off gas cylinder valve, the most again charging valve is unscrewed；
S4024: pull down connecting tube, shifts home onto gas cylinder dolly.
S403: entering automatic heating program, heating rate is 1.2mv/h, until material is smashed, now EF power is
11-15KW；
S404: after material is smashed, is cooled to after 0.5mv close intermediate frequency with the speed of-1.2mv/h, and after 12 hours, blow-on door prepares the
Secondary material；
The preparation of S5: seed crystal and adjustment, including following sub-step:
S501: seed crystal garnet crystal orients through strict, and deviation is less than 1 °, is cut into the square bar of 7.6 × 7.8mm；
S502: with boron carbide fine sand at the about 7mm of one end of seed crystal, grinds a symmetrical parallel semicircle little on the two sides of 7.8mm
Groove, makes seed crystal be contained on iridium bar vertical and feel have a little loosening to be advisable；
S503: after seed crystal milled, uses gasoline wash clean, then cleans with acetone, then adds detergent with tap water and cleans；Use after complete
The dilute hydrochloric acid of 1:5 soaks 5-10min, takes out and uses recycled water wash clean, and with available after alcohol wipe；
After S504: the second defective material installs, load onto seed crystal and mix up the concentricity of seed crystal, Concentricity tolerance≤1mm, weight fluctuation ＜
0.5g, preferably ＜ 0.2g；
After S505: seed crystal adjusts, adjust the viewing angle of observation panel 11, clean up burner hearth, banking door, evacuation, prepare
Material for the second time；
S6: for the second time material, inflate, preheat seed crystal, including following sub-step:
S601: the evacuation of material, inflation, temperature increasing for melting materials process have all operated with reference to material for the first time for the second time, heat up speed
Rate is 0.6mv/h；
S602: when Continental Europe table shows to 9mv, stops heating, opens mechanical pump evacuation, when being evacuated to-0.1MPa, stops taking out very
Sky, is filled with argon to 0.01MPa, then proceedes to heat up with 0.6mv/h, until material is completely melt；
S603: material needs to preheat seed crystal simultaneously, and the manual sinking seed crystal 2.5mm every 5 minutes, until seed crystal chaotropic face 1-2mm；Change
It should be noted that the speed of material fusing during material, prevent from heating up too fast too high；Meanwhile, once sinking seed crystal can not be too many, prevents
Seed crystal preheating is uneven and bursts.
S7: crystal growth, including following sub-step:
S701: sow, including:
S7011: constant temperature 0.5-1h after materialization is complete, then manually under shake seed crystal and sow, allow seed crystal contact with liquid level；
Start homoiothermic after S7012: seed crystal contact liquid level, carry out homoiothermic, constant temperature after each homoiothermic according to melt situation actual in stove
20min, and observe seed crystal head situation of change, as in figure 2 it is shown, when seed crystal head shrinks slightly, and formation half back taper is contacted with liquid level
Type, and when being always maintained at constant, show that temperature adjusts suitable；
S7013: temperature adjust suitable after, point 3 sinking seed crystal 2mm, each interval time 10-20min, sink seed for the last time
Constant temperature 0.5-1h after brilliant 0.5mm, can open and draw, rotating speed: 8-12 rev/min, pulling rate: 0.5-1mm/h；
S702: necking down: when starting to lift, makes temperature the most higher, allows seed crystal diameter micro-receipts about 1mm, entrance of lowering the temperature the most again
Shouldering；Purpose is that reducing seed crystal defect as far as possible extends to inside crystal.
S703: shouldering, isometrical, including:
The complete rear constant temperature 1h of S7031: necking down, can be introduced into pre-(Pre Auto) program automatically, manually set rotating speed: 10 revs/min, draw
Speed: 0.8mm/h；
S7032: in observation stove, crystal situation and crystal diameter and setting value walk power curve, if two curve deviations are little or crystal
Diametral curve is in slow shouldering state, can enter Automatic Control after inputting process parameters；
S7033: entering after automatically controlling, shouldering, isodiametric growth are grown by procedure auto-control temperature, and shouldering angle is
15-26 °, crystal diameter is 23-26 ° before φ 28mm, for 15-18 ° after reaching φ 28mm, proceed to isometrical after be 0 °；
S7034: when isodiametric growth to predetermined length, enters finishing phase；
S8: ending, comprises the following steps:
8.1 close pulling rate, and rotating speed, by automatically transferring to manually, is then log out automatic control program, and records gross weight.
8.2 manually on shake crystal (above shaking length to operate) by each stove specific length.
8.3 draw soon with 10mm/h, soon degree of elongation+above shake length=25mm；Start simultaneously at cooling, speed :-0.6mv/h,
Pulling post-tensioning velocity modulation soon is 0.5mm/h.
8.4 when starting to lower the temperature, and first closes UPS circuit board small power supply, more separately the big sky of stand-by power supply leaves.
8.5 when gross weight increases 200g, and pulling rate is adjusted to 2mm/h；When gross weight increases 400g, pulling rate is adjusted to 3mm/
h；This process can suitably reduce rotating speed.
8.6 as gross weight about 4.5Kg stall speed；If or found in temperature-fall period when seed crystal swings obvious, no matter
Gross weight is how many all should the speed of stall immediately.
8.7 stop pulling rate as gross weight about 9Kg；Or crystal shoulder φ 40mm expose insulation time, no matter weight is how many
All should stop pulling rate immediately.
8.8 when Continental Europe show be down to 0.5mv time, close intermediate frequency power supply.
8.9 after 12 hours, blow-on door, take out crystal.
S9: the maintenance that growth terminates:
After 9.1 take out crystal, clean burner hearth, remove dust stratification, and use alcohol wipe；And equipment is carried out hygiene and maintenance.
9.2 clean each insulation material, and install temperature field.
9.3 check whether mechanical rotation part has exception.
9.4 water routes are cleaned and check.
9.5 check that circuit, weighing system are the most normal.
If 9.6 temporarily do not use, answer closed furnace.
The above is only the preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form, is not to be taken as the eliminating to other embodiments, and can be used for other combinations various, amendment and environment, and can be at this
In the described contemplated scope of literary composition, it is modified by above-mentioned teaching or the technology of association area or knowledge.And those skilled in the art are entered
The change of row and change, the most all should be at the protection domains of claims of the present invention without departing from the spirit and scope of the present invention
In.
Claims (10)
1. crystal pull growth furnace temperature field structure, it is characterised in that: include aluminium oxide heat-preservation cylinder (1), zirconia brick heat-preservation cylinder
(2), iridium crucible (3), zirconium oxide crucible torr (4), aluminium oxide collet (5), the first zirconium oxide cover plate (6), aluminium oxide locating ring (7), oxygen
Change to be incubated on aluminum on inner core (8) and zirconium oxide and be incubated urceolus (9)；The perisporium of iridium crucible (3) is protected by zirconia brick the most successively
Temperature cylinder (2) and aluminium oxide heat-preservation cylinder (1) cladding；It is located at the bottom of the crucible of iridium crucible (3) on zirconium oxide crucible torr (4), zirconium oxide crucible torr (4),
Zirconia brick heat-preservation cylinder (2) and aluminium oxide heat-preservation cylinder (1) support respectively is on aluminium oxide collet (5)；The open top of iridium crucible (3)
Place is provided with the first zirconium oxide cover plate (6), is provided with aluminium oxide location between the first zirconium oxide cover plate (6) and aluminium oxide heat-preservation cylinder (1)
Ring (7), aluminium oxide is incubated insulation urceolus (9) on inner core (8) and zirconium oxide and is respectively arranged on the first zirconium oxide cover plate (6),
And insulation urceolus (9) is located on aluminium oxide locating ring (7) and aluminium oxide between insulation inner core (8) on zirconium oxide；Described oxidation
On aluminum be incubated inner core (8) and zirconium oxide on insulation urceolus (9) be also arranged above the second zirconium oxide cover plate (13), described oxidation
It is incubated insulation urceolus (9) on inner core (8) and zirconium oxide on aluminum and is the heat-preservation cylinder of reduction thickness.
Crystal pull the most according to claim 1 growth furnace temperature field structure, it is characterised in that: it is incubated on described aluminium oxide
The ratio being incubated urceolus (9) reduction thickness on inner core (8) and zirconium oxide is 30%-50%.
Crystal pull the most according to claim 1 growth furnace temperature field structure, it is characterised in that: also include induction coil (12),
The upper edge of iridium crucible (3) than on induction coil (12) dead ahead along exceeding 1 ~ 3mm, aluminium oxide heat-preservation cylinder (1) higher than induction coil (12) 30 ~
32mm。
Crystal pull the most according to claim 1 growth furnace temperature field structure, it is characterised in that: described iridium crucible (3) upper
Along than on zirconia brick heat-preservation cylinder (2) along low 5 ~ 8mm.
Crystal pull the most according to claim 1 growth furnace temperature field structure, it is characterised in that: described aluminium oxide locating ring
(7) being provided with foamed brick (10), foamed brick (10) is coated on zirconium oxide the outside of insulation urceolus (9).
Crystal pull the most according to claim 1 growth furnace temperature field structure, it is characterised in that: also include observation panel (11),
Observation panel (11) is located at the top of temperature field structure.
7. crystal pull growth technique, it is characterised in that comprise the following steps:
S1: prepare before shove charge；
S2: process iridium crucible；
S3: shove charge, charging, including following sub-step:
S301: the induction furnace to new clothes, first adjusts the levelness of induction coil (12), and induction coil (12) and seed rod is same
Heart degree, deviation should be less than 2mm；
S302: according to temperature field structure assembling temperature field, when dress temperature field, all of insulation material need to clean up without airborne dust, nothing
Temperature field can be loaded after falling slag；Adjust the concentricity of aluminium oxide heat-preservation cylinder (1), iridium crucible (3) and seed rod, deviation≤1mm；
S303: after clearing furnace, fire door is shut, prepares charging；
Before charging, the foreign material in cleaning iridium crucible (3), prevent foreign material from directly contacting with material, iridium crucible (3)；
Charging process wears altex glove, prevents secondary pollution；
After material installs, protect on the first zirconium oxide cover plate (6) of clean dust, the second zirconium oxide cover plate (13) and aluminium oxide with sweeping
It is incubated urceolus (9) on temperature inner core (8), zirconium oxide and installs heat-insulation system, adjust observation panel (11) angle, and with through processing
YAG crystal wafer cover observation panel (11)；
Check again for induction coil (12) with or without leaking, turn-to-turn short circuit, clean banking door after burner hearth, evacuation；
S4: material for the first time, including following sub-step:
S401: start mechanical pump, slowly open vacuum valve, after vacuum is evacuated to 5Pa, opens intermediate frequency power supply, manually rises Continental Europe table
OP to 80V, rises DC voltage to 100V to DC voltage after 1h；
S402: be heated to 100V, after vacuum is evacuated to 5Pa again, closes vacuum valve, closes mechanical pump, manually by Continental Europe OP
After value is down to 0, starts to be filled with argon extremely-0.01MPa, more manually rise the show value before the extremely inflation of Continental Europe OP value；
S403: entering automatic heating program, heating rate is 1.2mv/h, until material is smashed, now EF power is 11-
15KW；
S404: after material is smashed, is cooled to after 0.5mv close intermediate frequency with the speed of-1.2mv/h, and after 12 hours, blow-on door prepares the
Secondary material；
The preparation of S5: seed crystal and adjustment, including following sub-step:
S501: seed crystal garnet crystal orients through strict, and deviation is less than 1 °, the side's of being cut into bar；
S502: grind a symmetrical parallel semicircle sulculus with boron carbide fine sand two sides at one end 6-8mm of seed crystal, make seed crystal
It is contained on iridium bar vertical and has a little loosening；
S503: after seed crystal milled, uses gasoline wash clean, then cleans with acetone, then adds detergent with tap water and cleans；Use after complete
The dilute hydrochloric acid of 1:5 soaks 5-10min, takes out and uses recycled water wash clean, and with available after alcohol wipe；
After S504: the second defective material installs, load onto seed crystal and mix up the concentricity of seed crystal, Concentricity tolerance≤1mm, weight fluctuation ＜
0.2-0.5g；
After S505: seed crystal adjusts, adjust the viewing angle of observation panel (11), clean up burner hearth, banking door, evacuation, standard
Standby second time material；
S6: for the second time material, inflate, preheat seed crystal, including following sub-step:
S601: the evacuation of material, inflation, temperature increasing for melting materials process have all operated with reference to material for the first time for the second time, heat up speed
Rate is 0.6mv/h；
S602: when Continental Europe table shows to 9mv, stops heating, opens mechanical pump evacuation, when being evacuated to-0.1MPa, stops taking out very
Sky, is filled with argon to 0.01MPa, then proceedes to heat up with 0.6mv/h, until material is completely melt；
S603: material needs to preheat seed crystal simultaneously, and the manual sinking seed crystal 2.5mm every 5 minutes, until seed crystal chaotropic face 1-2mm；
S7: crystal growth, including following sub-step:
S701: sow, including:
S7011: constant temperature 0.5-1h after materialization is complete, then manually under shake seed crystal and sow, allow seed crystal contact with liquid level；
Start homoiothermic after S7012: seed crystal contact liquid level, carry out homoiothermic, constant temperature after each homoiothermic according to melt situation actual in stove
20min, and observe seed crystal head situation of change, when seed crystal head shrinks slightly, and contact formation half inverted cone-shaped with liquid level, and protect always
When holding constant, show that temperature adjusts suitable；
S7013: temperature adjust suitable after, point 3 sinking seed crystal 2mm, each interval time 10-20min, sink seed for the last time
Constant temperature 0.5-1h after brilliant 0.5mm, can open and draw, rotating speed: 8-12 rev/min, pulling rate: 0.5-1mm/h；
S702: necking down: when starting to lift, makes temperature the most higher, allows seed crystal diameter micro-receipts about 1mm, entrance of lowering the temperature the most again
Shouldering；
S703: shouldering, isometrical, including:
The complete rear constant temperature 1h of S7031: necking down, setting speed: 8-12 rev/min, pulling rate: 0.5-1mm/h；
S7032: in observation stove, crystal situation and crystal diameter and setting value walk power curve, if two curve deviations are little or crystal
Diametral curve is in slow shouldering state, can enter Automatic Control after inputting process parameters；
S7033: entering after automatically controlling, shouldering, isodiametric growth are grown by procedure auto-control temperature, and shouldering angle is
15-26 °, crystal diameter is 23-26 ° before φ 28mm, for 15-18 ° after reaching φ 28mm, proceed to isometrical after be 0 °；
S7034: when isodiametric growth to predetermined length, enters finishing phase；
S8: ending.
Crystal pull growth technique the most according to claim 7, it is characterised in that: described step S1 includes brilliant liter/crystalline substance
Turn check step, weighing system check step, vacuum check step, water route and channel check step, Continental Europe systems inspection step,
The combination of any one or more in induction coil inspection step and mechanical pump inspection step:
(1) brilliant liter/crystalline substance turn checks: the brilliant liter of detection, crystalline substance turn the most properly functioning, and fluctuation of speed scope is normal ± 0.1, pulling rate
Fluctuation range is normal ± 0.01, and crystalline substance turns non-jitter, and brilliant liter is without creeping phenomenon；
(2) weighing system inspection: detection weighing system is the most properly functioning, and weight fluctuation ＜ 0.2g is normal；
(3) vacuum inspection, including following sub-step:
SS1: closed furnace door, checks whether venting valve, charging valve close；
SS2: start mechanical pump, slowly open vacuum valve；
SS3: observe vacuometer, whether detection furnace pressure can reach below 5Pa, and maintain a period of time；
(4) water route and channel check: check whether each cooling water channel is opened before starting the heating, hydraulic pressure is the most normal: body of heater water
Pressure is 0.04-0.06MPa, and induction coil hydraulic pressure is 0.25-0.3MPa；Check circuit whether normal operation；
(5) Continental Europe systems inspection: logical upper Continental Europe power supply, Continental Europe table, to automatically, arranges auto linear heating schedule, and observation program is
No properly functioning, Continental Europe table mv value displays whether normally；
(6) induction coil inspection: check whether induction coil leaks, with or without the phenomenon of turn-to-turn short circuit；
(7) mechanical pump inspection: check whether the oil of mechanical pump adds properly, in terms of observation panel, oil is added to the half of observation panel；
Open mechanical pump power supply, see that operating is the most normal.
Crystal pull growth technique the most according to claim 7, it is characterised in that: described step S2 includes following sub-step
Rapid:
S201: after the dilute hydrochloric acid of use 1:5 is to cleaning 0.5-1h inside and outside iridium crucible, cleans up with distilled water and dry, and use ethanol
Wiped clean is standby；
Carrying out vacuum sky burning before the charging of S202: iridium crucible to process, vacuum sky burning processes and includes following sub-step:
S2021: mix up the concentricity rear enclosed fire door of iridium crucible and seed rod, closes venting valve；
S2022: start mechanical pump, slowly opens vacuum valve, starts evacuation；
S2023: after vacuum is evacuated to 5Pa, starts intermediate frequency power supply, first opens control loop, opens major loop again, manually rises Continental Europe table OP value
To DC voltage to 80V；After 1h, liter DC voltage is to 100V, utilizes JPG Automatic Program to heat up, heating rate after half an hour
For 1.2mv/h；
S2024: observe iridium crucible sky in stove and burn situation, when with the naked eye watching iridium crucible and feeling the most dazzling, stopping heating up enters constant temperature
State, now EF power about 7-8KW；After constant temperature 2h, starting cooling automatically, rate of temperature fall is-1.2mv/h, is cooled to 0.5mv
Intermediate frequency power supply can be closed, close mechanical pump；
S2025: closing intermediate frequency power supply order: Continental Europe furnishing is manual, OP value is down to 0, closes major loop, closes and controls loop, closes power supply
Plug-in strip；
S2026: fire door can be opened after closing intermediate frequency power supply 12h.
Crystal pull growth technique the most according to claim 7, it is characterised in that: it is filled with argon described in step S402
Step includes:
S4021: charging valve is unscrewed, then open gas cylinder valve；
S4022: slowly charging valve is progressively tightened, first aerofluxus, after being emptied by the air in connecting tube, reconnect inflation air inlet
Pipe；
S4023: slowly open inflation connecting valve, after making stove internal gas pressure rise to specify air pressure, first closes inflation connecting valve,
Turn off gas cylinder valve, the most again charging valve is unscrewed；
S4024: pull down connecting tube, shifts home onto gas cylinder dolly.
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| CN108893780A (en) * | 2018-07-19 | 2018-11-27 | 中山大学 | A kind of crystal growing apparatus and the double-doped LuAG crystal of a kind of Er, Yb and preparation method thereof |
| EP3851562A4 (en) * | 2019-08-21 | 2022-02-09 | Meishan Boya Advanced Materials Co., Ltd. | Multi-component garnet-structured scintillation crystal growth method and equipment |
| CN114250515A (en) * | 2021-12-13 | 2022-03-29 | 长飞光纤光缆股份有限公司 | Calcium-magnesium-zirconium-doped gadolinium-gallium garnet crystal, preparation method, application and temperature field thereof |
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| CN117552110A (en) * | 2024-01-02 | 2024-02-13 | 内蒙古晶环电子材料有限公司 | Heat preservation structure and crystal growth furnace |
| CN117646279A (en) * | 2024-01-30 | 2024-03-05 | 常州臻晶半导体有限公司 | Double-heater device for growing silicon carbide single crystal by liquid phase method and method thereof |
| CN117646279B (en) * | 2024-01-30 | 2024-04-05 | 常州臻晶半导体有限公司 | Double-heater device for growing silicon carbide single crystal by liquid phase method and method thereof |
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Application publication date: 20161109 |